CN109750509B - Anti-ultraviolet hydrophobic flame-retardant real silk fabric and preparation method thereof - Google Patents
Anti-ultraviolet hydrophobic flame-retardant real silk fabric and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a preparation method of an anti-ultraviolet hydrophobic flame-retardant real silk fabric, which comprises the following steps: soaking the real silk fabric in dopamine aqueous solution containing ferrous ions at 40-50 ℃, after complete reaction, adding peroxide and continuing to process for 40min at 50 ℃; after washing and drying, the treated fabric was washed at 0.1kg/cm2‑1kg/cm2And (3) padding multivalent metal ions under pressure, and baking to obtain the anti-ultraviolet hydrophobic flame-retardant real silk fabric. The anti-ultraviolet hydrophobic flame-retardant real silk fabric and the preparation method thereof have the advantages of environment-friendly and easily-obtained raw materials, simple method, mild treatment conditions, low energy consumption and high efficiency, are particularly suitable for industrial production, and integrate the anti-ultraviolet, hydrophobic and flame-retardant effects into a whole.
Description
Technical Field
The invention relates to the technical field of textile after-finishing, in particular to an anti-ultraviolet hydrophobic flame-retardant real silk fabric and a preparation method thereof.
Background
The real silk fabric has gorgeous luster and comfortable hand feeling, and is widely used for high-grade textile fabrics, such as bedding, curtains, wall cloth, automotive interiors and the like. Real silk fabrics are flammable, and personal and property losses caused by textile fires gradually increase every year. Inspired by nature, the super-hydrophobic surface attracts people's attention, and the hydrophobic surface has the characteristics of water repellency, self-cleaning, no icing, difficult decay and the like, and has wide prospects in various fields. If the textile has multiple functions while keeping the color, the application range of the textile is inevitably widened, and the additional value of the textile is greatly increased.
The patent CN 201710558475.6 discloses an anti-ultraviolet soft finishing agent for textiles and a preparation method thereof, methyl hydrogen-containing silicone oil, acrylamide and allyl polyoxyethylene polyoxypropylene ether are used as raw materials, chloroplatinic acid is used as a catalyst to synthesize an intermediate I, cyanuric chloride and resorcinol are synthesized into an intermediate II under the catalysis of aluminum trichloride, and finally the intermediate I and the intermediate II are reacted to obtain the anti-ultraviolet soft finishing agent, so that the anti-ultraviolet capability of the textiles is improved. The patent CN201610801962.6 discloses a super-hydrophobic and anti-ultraviolet finishing agent for textiles and a preparation method thereof, wherein tetraethoxysilane is used as a raw material to prepare silica sol, 3-propyltrimethoxysilane is used to modify the silica sol, and the obtained modified silica sol with double bonds is reacted with long-chain aliphatic hydrocarbon acrylate and 2-hydroxy-4-methacryloxy benzophenone to successfully prepare the super-hydrophobic and anti-ultraviolet finishing agent. Patent CN 201610826073.5 discloses a preparation method of flame-retardant hydrophobic wool fabric, which comprises the steps of firstly preparing flame-retardant doped sol, then adding a hydrophobic finishing agent to prepare a flame-retardant hydrophobic solution, and finally finishing the fabric. However, in the prior art, part of products have single functionality, and when another part of products are prepared, the consumption of chemicals is large, part of chemicals contain or potentially contain toxicity, and the production process is complicated, long in time consumption and low in efficiency, so that the method is not suitable for large-scale production.
Therefore, a simple, convenient, environment-friendly and low-cost method for preparing the functional real silk fabric integrating the ultraviolet resistance, the hydrophobic property and the flame retardance is needed.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide the anti-ultraviolet hydrophobic flame-retardant real silk fabric and the preparation method thereof, the raw materials are environment-friendly and easy to obtain, the treatment temperature is low, the energy consumption is low, the operation is simple, the time consumption is short, the efficiency is high, the industrial production is convenient, and the product integrates the anti-ultraviolet, hydrophobic and flame-retardant effects.
In one aspect, the invention provides a preparation method of an anti-ultraviolet hydrophobic flame-retardant real silk fabric, which comprises the following steps:
(1) soaking the real silk fabric in an aqueous solution containing ferrous salt and dopamine at a bath ratio of 1:20-1:100 at 40-50 ℃ for reaction for 10-20min, then adding a peroxide aqueous solution into the real silk fabric, and continuing the reaction for 30-40 min; washing the fabric after the reaction is completed, and then drying at 50-80 ℃;
(2) padding the dried silk fabric by using an aqueous solution containing polyvalent metal ions, wherein the padding treatment is a two-padding and two-rolling method, and the padding treatment pressure is 0.1kg/cm2-1kg/cm2；
(3) And after padding treatment, pre-drying the fabric for 5min at 60-70 ℃, and then raising the temperature to 80-90 ℃ for baking for 4min-10min to obtain the anti-ultraviolet hydrophobic flame-retardant real silk fabric.
Further, in the step (1), the concentration of the ferrous salt in the aqueous solution is 1.5mmol/L-4 mmol/L.
Further, in the step (1), the concentration of the dopamine in the aqueous solution is 2g/L-10 g/L.
Further, in the step (1), the ferrous salt is one or more of ferrous sulfate, ferrous chloride, ferrous nitrate, ferrous acetate, ferrous lactate, ferrous bromide and ferrous glycinate.
Further, in the step (1), the concentration of the peroxide aqueous solution is 8mmol/L-16 mmol/L.
Further, in the step (1), the peroxide is one or more of sodium perborate, potassium perborate, sodium persulfate and potassium persulfate.
Further, in the step (2), the pH of the aqueous solution containing polyvalent metal ions is 3 to 6.
Further, in the step (2), the polyvalent metal ions are one or more of ferrous ions, ferric ions, copper ions and zinc ions.
Further, in the step (2), the concentration of the polyvalent metal ion-containing aqueous solution is 20mmol/L to 80 mmol/L.
Further, in the step (2), during padding treatment, the dried silk fabric is soaked in the aqueous solution containing the polyvalent metal ions for 1min to 2min, and then padding treatment is carried out.
On the other hand, the invention also provides the anti-ultraviolet hydrophobic flame-retardant real silk fabric prepared by the method.
The contact angle of the anti-ultraviolet hydrophobic flame-retardant real silk fabric to water drops is larger than 145 degrees, the anti-ultraviolet UPF value is more than 30, and the vertical burning damage length is within 15 cm. Has good stability and strong water washing resistance.
The principle of the invention is as follows:
under the condition of ferrous ion catalysis, peroxide generates active oxygen molecules to promote the rapid polymerization of dopamine, and a polydopamine coating is formed on the surface of real silk. When the mangle containing the polyvalent metal ions is treated, phenolic hydroxyl in the molecular structure of the polydopamine adsorbs the polyvalent metal ions through strong chelation, the polydopamine is forcedly hydrolyzed under the weak acid condition to form oxyhydroxide, and then the oxyhydroxide is dried and dehydrated to form particles to cover the surface of the real silk fabric to form a nano-particle coating. The nano-particle coating has a hydrophobic nano-structure, and the ultraviolet resistance of polydopamine and the non-combustible property of the metal oxide particles are added, so that the fabric has ultraviolet resistance, flame retardance and hydrophobicity.
By the scheme, the invention at least has the following advantages:
(1) in the preparation method of the anti-ultraviolet hydrophobic flame-retardant real silk fabric, dopamine is polymerized in a rapid oxidative polymerization mode, so that the polymerization rate of the dopamine is greatly increased. The defects of long time consumption (usually 24h) and low efficiency of the traditional dopamine polymerization method are overcome.
(2) The polydopamine in the invention adsorbs polyvalent metal ions as mineralization sites through chelation on one hand, and enables oxyhydroxide to be stably fixed on the surface of the fabric by utilizing extremely strong interface adhesion performance on the other hand. The defects of non-durability and low fastness of the traditional functional fabric are overcome; the used raw materials are green, environment-friendly and pollution-free, and accord with the ecological concept of energy conservation and emission reduction.
(3) The preparation method of the anti-ultraviolet hydrophobic flame-retardant real silk fabric has the advantages of low treatment temperature, low energy consumption, simple operation, short time consumption, high efficiency and convenience for industrial production, and the product integrates anti-ultraviolet, hydrophobic and flame-retardant effects, so that the application range of real silk can be expanded, and the additional value of the product is increased.
(4) The super-hydrophobic anti-ultraviolet flame-retardant real silk fabric prepared by the method has a contact angle to water drops larger than 145 degrees, an anti-ultraviolet UPF value of more than 30 and a vertical burning damage length within 15 cm. Has good stability and strong water washing resistance.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood and to be implemented in accordance with the content of the description, the following detailed description is given with reference to the embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is a scanning electron microscope image of a real silk fabric before and after being treated by the method of the first embodiment;
FIG. 2 is a graph of the contact angle of a real silk fabric treated by the method of the first embodiment;
FIG. 3 is a vertical burning chart of real silk fabric before and after being treated by the method of the first embodiment.
Detailed Description
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example one
10 × 10cm2The silk fabric is immersed in 150mL of aqueous solution, 0.3g of dopamine and 0.05g of ferrous sulfate heptahydrate are added into the aqueous solution, the mixture is shaken and reacted for 20min at a constant temperature in a shaking dyeing machine at 50 ℃, and then 0.37g of sodium perborate tetrahydrate is added into the mixture, and the reaction is continued for 40 min. The fabric was removed, washed to remove unreacted reagents and then dried at 80 ℃ for 20 min.
Soaking the dried real silk fabric in 40mmol/L ferrous sulfate heptahydrate water solution (pH value of 3) for 2min, and then soaking the real silk fabric in 0.5kg/cm2And (4) carrying out liquid rolling treatment under pressure. Re-immersing the treated fabric in40mmol/L ferrous sulfate heptahydrate aqueous solution (pH 3) for 2min, then 0.5kg/cm2And (4) carrying out liquid rolling treatment under pressure.
And after padding treatment, taking out the fabric, washing to remove unreacted reagents, pre-drying at 70 ℃ for 5min, and then raising the temperature to 90 ℃ for baking for 10min to obtain the anti-ultraviolet hydrophobic flame-retardant real silk fabric.
Table 1 shows the uvioresistant performance of the fabric prepared in this example, and the UVA of the treated real silk fabric is less than 4%, and the UPF is greater than 30, which indicates that the fabric has a certain uvioresistant performance. FIG. 1 shows the surface morphology of real silk fabric before and after treatment, as can be seen from FIG. 1(a), the fiber surface before treatment is smooth, and as can be seen from FIG. 1(b), a large amount of particles are aggregated on the fiber surface after treatment, and the surface roughness is increased; FIG. 2 shows that the contact angle of the uvioresistant hydrophobic real silk fabric prepared in the embodiment to water reaches 155 degrees. FIG. 3 shows the vertical burning condition of real silk fabric prepared by the embodiment, and the damage length is 11.2 cm.
TABLE 1 uvioresistant performance of uvioresistant hydrophobic flame-retardant real silk fabric
Example two
10 × 10cm2Soaking the real silk fabric into 150mL of aqueous solution, adding 1.0g of dopamine and 0.15g of ferrous bromide, carrying out shake reaction at 50 ℃ for 10min in a constant-temperature shake dyeing machine, then adding 0.5g of potassium persulfate, and continuing the reaction for 40 min. The fabric was removed, washed to remove unreacted reagents and then dried at 80 ℃ for 20 min.
Soaking the dried real silk fabric in 80mmol/L anhydrous copper sulfate water solution (pH of 6) for 2min, and adding into the solution at 0.5kg/cm2And (4) carrying out liquid rolling treatment under pressure. The treated fabric was again immersed in 80mmol/L of anhydrous copper sulfate aqueous solution (pH 6) for 2min, and then at 0.5kg/cm2And (4) carrying out liquid rolling treatment under pressure.
And after padding treatment, taking out the fabric, washing to remove unreacted reagents, pre-drying at 70 ℃ for 5min, and then raising the temperature to 80 ℃ for baking for 10min to obtain the anti-ultraviolet hydrophobic flame-retardant real silk fabric.
EXAMPLE III
10 × 10cm2Soaking the real silk fabric into 150mL of aqueous solution, adding 0.45g of dopamine and 0.1g of ferrous chloride, carrying out shake reaction at 50 ℃ for 15min in a constant-temperature shake dyeing machine, then adding 0.5g of potassium perborate, and continuing the reaction for 38 min. The fabric was removed, washed to remove unreacted reagents and then dried at 80 ℃ for 20 min.
Soaking the dried real silk fabric in 80mmol/L ferric chloride hexahydrate aqueous solution (pH value of 5) for 2min, and then soaking the real silk fabric in 1kg/cm2Mangling under pressure the treated fabric was again immersed in an aqueous solution of 80mmol/L iron chloride hexahydrate at pH 5 for 2min and then at 1kg/cm2And (4) carrying out liquid rolling treatment under pressure.
And after padding treatment, taking out the fabric, washing to remove unreacted reagents, pre-drying at 67 ℃ for 5min, and then raising the temperature to 80 ℃ for baking for 10min to obtain the anti-ultraviolet hydrophobic flame-retardant real silk fabric.
Example four
10 × 10cm2Soaking the real silk fabric into 150mL of aqueous solution, adding 0.3g of dopamine and 0.05g of ferrous acetate, carrying out shake reaction at 50 ℃ for 20min in a constant-temperature shake dyeing machine, then adding 0.5g of potassium persulfate, and continuing the reaction for 40 min. The fabric was removed, washed to remove unreacted reagents and then dried at 80 ℃ for 20 min.
Soaking the dried real silk fabric in 60mmol/L zinc chloride water solution (pH value of 5) for 2min, and adding into the solution at 0.5kg/cm2And (4) carrying out liquid rolling treatment under pressure. The treated fabric was again immersed in a 60mmol/L aqueous solution of zinc chloride (pH 5) for 2min and then at 0.5kg/cm2And (4) carrying out liquid rolling treatment under pressure.
And after padding treatment, taking out the fabric, washing to remove unreacted reagents, pre-drying at 69 ℃ for 5min, and then raising the temperature to 80 ℃ for baking for 10min to obtain the anti-ultraviolet hydrophobic flame-retardant real silk fabric.
EXAMPLE five
10 × 10cm2The real silk fabric of (1) was immersed in 150mL of an aqueous solution, and then 0.3g of dopamine and 0.05g of sulfuric acid sulfite heptahydrate were added theretoAnd (3) oscillating iron at 50 ℃ in a constant-temperature oscillation dyeing machine for 20min, adding 0.37g of sodium perborate tetrahydrate, and continuing to react for 35 min. The fabric was removed, washed to remove unreacted reagents and then dried at 80 ℃ for 20 min.
Soaking the dried real silk fabric in an aqueous solution (pH 4) containing 80mmol/L ferrous sulfate heptahydrate and 60mmol/L anhydrous copper sulfate for 2min, and adding into a container at a concentration of 0.5kg/cm2And (4) carrying out liquid rolling treatment under pressure. The treated fabric was again immersed in an aqueous solution (pH 4) containing 80mmol/L of ferrous sulfate heptahydrate and 60mmol/L of anhydrous copper sulfate for 2min, and then at 0.5kg/cm2And (4) carrying out liquid rolling treatment under pressure.
And after padding treatment, taking out the fabric, washing to remove unreacted reagents, pre-drying at 65 ℃ for 5min, and then raising the temperature to 80 ℃ for baking for 10min to obtain the anti-ultraviolet hydrophobic flame-retardant real silk fabric.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (8)
1. The preparation method of the anti-ultraviolet hydrophobic flame-retardant real silk fabric is characterized by comprising the following steps of:
(1) soaking the real silk fabric in an aqueous solution containing ferrous salt and dopamine at a bath ratio of 1:20-1:100 at 40-50 ℃ for reaction for 10-20min, then adding a peroxide aqueous solution into the real silk fabric, and continuing the reaction for 30-40 min; washing the fabric after the reaction is completed, and then drying at 50-80 ℃; in the aqueous solution, the concentration of ferrous salt is 1.5mmol/L-4 mmol/L;
(2) padding the dried silk fabric by using an aqueous solution containing polyvalent metal ions, wherein the padding treatment is a two-padding and two-rolling method, and the padding treatment pressure is 0.1kg/cm2-1kg/cm2(ii) a The pH value of the aqueous solution containing the polyvalent metal ions is 3-6;
(3) and after padding treatment, pre-drying the fabric for 5min at 60-70 ℃, and then raising the temperature to 80-90 ℃ for baking for 4min-10min to obtain the anti-ultraviolet hydrophobic flame-retardant real silk fabric.
2. The method of claim 1, wherein: in the step (1), the concentration of the dopamine in the aqueous solution is 2g/L-10 g/L.
3. The method of claim 1, wherein: in the step (1), the ferrous salt is one or more of ferrous sulfate, ferrous chloride, ferrous nitrate, ferrous acetate, ferrous lactate, ferrous bromide and ferrous glycinate.
4. The method of claim 1, wherein: in the step (1), the concentration of the peroxide aqueous solution is 8mmol/L-16 mmol/L.
5. The method of claim 1, wherein: in the step (1), the peroxide is one or more of sodium perborate, potassium perborate, sodium persulfate and potassium persulfate.
6. The method of claim 1, wherein: in the step (2), the polyvalent metal ions are one or more of ferrous ions, ferric ions, copper ions and zinc ions.
7. The method of claim 1, wherein: in the step (2), the concentration of the polyvalent metal ion-containing aqueous solution is 20mmol/L to 80 mmol/L.
8. An uvioresistant hydrophobic flame-retardant real silk fabric obtained by the preparation method according to any one of claims 1 to 7.
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| CN108729231A (en) * | 2018-06-27 | 2018-11-02 | 南通纺织丝绸产业技术研究院 | Coloured uvioresistant hydrophobic fabric and preparation method thereof |
| CN108893990A (en) * | 2018-04-19 | 2018-11-27 | 苏州大学 | A kind of multi-functional preparation method containing silk fabric |
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| CN108893990A (en) * | 2018-04-19 | 2018-11-27 | 苏州大学 | A kind of multi-functional preparation method containing silk fabric |
| CN108729231A (en) * | 2018-06-27 | 2018-11-02 | 南通纺织丝绸产业技术研究院 | Coloured uvioresistant hydrophobic fabric and preparation method thereof |
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| 基于多巴胺表面改性的蚕丝和锦纶织物阻燃整理;匡小慧;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》;20190115;B024-292 * |
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